WO2014180333A1 - Matériau composite de batterie et procédé de fabrication de précurseur de celui-ci - Google Patents

Matériau composite de batterie et procédé de fabrication de précurseur de celui-ci Download PDF

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Publication number
WO2014180333A1
WO2014180333A1 PCT/CN2014/077080 CN2014077080W WO2014180333A1 WO 2014180333 A1 WO2014180333 A1 WO 2014180333A1 CN 2014077080 W CN2014077080 W CN 2014077080W WO 2014180333 A1 WO2014180333 A1 WO 2014180333A1
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Prior art keywords
phosphoric acid
battery composite
compound
solution
precursor
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PCT/CN2014/077080
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English (en)
Chinese (zh)
Inventor
洪辰宗
林季延
黄安锋
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台湾立凯电能科技股份有限公司
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Priority to CN201480022089.XA priority Critical patent/CN105409033B/zh
Priority to CA2911458A priority patent/CA2911458C/fr
Priority to EP14794480.5A priority patent/EP2996179A4/fr
Priority to KR1020157034869A priority patent/KR101787229B1/ko
Priority to JP2016512215A priority patent/JP6239095B2/ja
Priority to US14/889,418 priority patent/US10236512B2/en
Publication of WO2014180333A1 publication Critical patent/WO2014180333A1/fr

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/45—Phosphates containing plural metal, or metal and ammonium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/049—Manufacturing of an active layer by chemical means
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the invention relates to a preparation method, in particular to a preparation method of a battery composite material. Background technique
  • lithium-ion batteries have potential for development, and they have become the mainstream in the market, including high volumetric capacitance, rechargeable, and good cycle charge and discharge.
  • lithium ion batteries using lithium iron phosphate as a positive electrode material have attracted the most attention.
  • the battery with lithium iron phosphate (LiFeP0 4 , abbreviated as LFP) as the positive electrode material has the advantages of large current, long cycle life, oxidation resistance, acid corrosion resistance, etc., and does not release oxygen during charging and discharging, and there is no risk of explosion. It exists, so it is considered to be one of the most promising lithium ion battery cathode materials.
  • the object of the present invention is to provide a method for preparing a battery composite material, which can avoid the agglomeration effect between the finished powders during the heat treatment by diffusing the manganese source into the iron source, thereby solving the existing process for preparing the lithium iron phosphate compound. Due to the increase in the particle size of the finished powder, the electrical properties are degraded.
  • Another object of the present invention is to provide a method for preparing a battery composite material, wherein a manganese source is diffused into an iron source, and a manganese atom is surrounded and coated with iron atoms, which facilitates the reaction and prevents the finished powder from being heat treated.
  • the agglomeration effect occurs in the process, thereby achieving the advantage of improving the electrical performance of the battery.
  • Another object of the present invention is to provide a method for preparing a battery composite material, which is prepared by selecting a particle size of an iron source and a ratio of a manganese source ratio to prepare a battery composite material having an ideal electrical performance according to actual needs.
  • a broader embodiment of the present invention provides a method for preparing a battery composite, comprising at least the steps of: (a) providing an iron compound, a phosphoric acid, a manganese compound, a lithium compound, and a carbon source, wherein the phosphoric acid The chemical formula is H 3 P0 4; (b) the iron compound is mixed with deionized water and stirred, and then the phosphoric acid is added and stirred to form the first a phosphoric acid solution, adding a first amount of the manganese compound to the first phosphoric acid solution, and continuously reacting the manganese compound with the first phosphoric acid solution for a first time to form the first product solution; (c) At least the first product solution, the carbon source, and the lithium compound are reacted to form a precursor, the carbon source being a saccharide, an organic compound, a polymer or a polymer material; and (d) heat treating the precursor To generate the battery composite material, the chemical formula of the battery composite is Li
  • another broad embodiment of the present invention provides a method for preparing a battery composite, comprising at least the steps of: (a) providing an iron compound, phosphoric acid, MnCO 3 , LiOH, and a carbon source, wherein the phosphoric acid The chemical formula is H 3 P0 4; (b) mixing and stirring the iron compound and deionized water, adding the phosphoric acid and stirring to form a first phosphoric acid solution, and adding a first amount of the first phosphoric acid solution MnC0 3, MnC0 3 the reaction was continued for the first time to a first acid solution to form a first product of the solution; (c) reacting the first product in solution, the carbon source and LiOH, to produce a precursor, the carbon source being a saccharide, an organic compound, a polymer or a polymer material; and (d) heat treating the precursor to form the battery composite, the chemical formula of the battery composite being LiFe x M ni — x P0 4, wherein X is
  • another broad embodiment of the present invention provides a method for preparing a precursor of a battery composite, comprising at least the steps of: reacting iron with a compound that releases manganese ions in an aqueous phosphoric acid solution to form a first a product solution; reacting the first product solution with a compound that releases lithium ions in an aqueous phosphoric acid solution to form a precursor solution; and drying the precursor solution to obtain a precursor of the battery composite material, the precursor
  • the chemical formula is LiFe x M ni - x P0 4 , where X is greater than zero.
  • FIG. 1 is a flow chart of a method for preparing a battery composite material according to a preferred embodiment of the present invention.
  • step S300 is a detailed flow chart of step S300 of the method for preparing a battery composite material of the present invention.
  • Fig. 3 is a X-ray diffraction analysis chart of the finished powder obtained in Example 1.
  • Fig. 4 is a X-ray diffraction analysis diagram of the finished powder obtained in Example 2.
  • Fig. 5 is a scanning electron microscope analysis chart of the finished powder obtained in Example 1.
  • Fig. 6 is a scanning electron microscope analysis chart of the finished powder obtained in Example 2.
  • Fig. 7 is a graph showing the charge and discharge characteristics of a button type battery made of the finished powder obtained by the method for producing a battery composite material of Example 1.
  • Fig. 8 is a graph showing the charge and discharge characteristics of a button type battery made of the finished powder obtained by the method for producing a battery composite material of Example 2.
  • FIG. 1 is a flow chart of a method for preparing a battery composite material according to a preferred embodiment of the present invention.
  • the preparation method of the battery composite material of the present invention comprises the following steps: First, as shown in step S100, an iron compound, a phosphoric acid, a manganese compound and a lithium compound are provided. Among them, the chemical formula of phosphoric acid is H 3 P0 4 .
  • the manganese compound may be, but not limited to, manganese carbonate (MnCO 3 ), manganese oxide (MnO), or other compound containing manganese and releasing manganese ions in an aqueous phosphoric acid solution, and manganese carbonate is preferred.
  • the lithium compound may be, but not limited to, lithium hydroxide (LiOH), lithium carbonate (Li 2 CO 3 ) or other compound containing lithium and capable of releasing lithium ions in an aqueous phosphoric acid solution, and lithium hydroxide is preferred.
  • LiOH lithium hydroxide
  • Li 2 CO 3 lithium carbonate
  • lithium hydroxide lithium hydroxide
  • the iron compound may be selected from, but not limited to, Fe 7 (P0 4 ) 6 , FeP (V 2 H 2 0, LiFeP 0 4 , Fe 2 0 3
  • compounds such as Fe 7 (P0 4 ) 6 , FeP0 4 -2H 2 0 and LiFeP 0 4 are preferred iron sources.
  • the iron compound and the deionized water are mixed and stirred to initially disperse the iron compound in the deionized water.
  • at least 85% by weight of phosphoric acid is added and stirred to further uniformly disperse the iron source to form a first phosphoric acid solution.
  • a first amount of the manganese compound is added to the first phosphoric acid solution, and the manganese compound is continuously reacted with the first phosphoric acid solution for a first time to form a first product solution.
  • an iron compound is used as an iron source, and the dispersibility of the iron compound in deionized water is increased by phosphoric acid to promote the subsequent reaction.
  • the first product solution is a solution containing an iron compound, a manganese ion, and a phosphate ion.
  • the phosphate ions contained in the first phosphoric acid solution increase the degree of dissociation of the manganese compound and uniformly distribute the manganese ions in the first product solution.
  • the first time that the manganese compound and the first phosphoric acid solution are continuously reacted is at least 24 hours, and preferably 24 hours, but not limited thereto, according to the phosphoric acid contained in the first phosphoric acid solution. The root concentration is adjusted.
  • the reaction is carried out with at least a first product solution, a carbon source, and a lithium compound to produce a precursor.
  • the carbon source may be, but not limited to, a saccharide, an organic compound, a polymer or a polymer material, and the saccharide may be at least one of fructose or lactose.
  • the precursor is heat treated to form a battery composite.
  • the step S300 further comprises reacting an oxide of a transition metal with the first product solution, the carbon source, and the lithium compound, and generating LiFe x M ni - 0 containing the metal oxide in the step S400. 4 , or nano metal oxide co-crystallized lithium iron phosphate manganese compound (LFMP-NC0), the chemical formula is LiFe x M ni - x P (V ⁇ , where ⁇ is greater than or equal to 1, ⁇ is a transition metal oxide,
  • the transition metal can be, but is not limited to, vanadium pentoxide (V 2 0 5 ).
  • FIG. 2 is a detailed flowchart of step S300 of the method for preparing a battery composite material of the present invention.
  • a lithium compound, a carbon source and a dispersing agent are added to the first product solution to form a second product solution.
  • the dispersing agent can be a nonionic surfactant, For example, Triton X-100.
  • a second polishing action is performed on the second product solution to generate a precursor solution.
  • the grinding operation is performed by a ball mill, for example, at a rotation speed of 450 rpm to 600 rpm for one hour, but not limited thereto.
  • step S303 the precursor solution is dried to remove excess water to form a preliminary dried precursor.
  • the preliminary dried precursor is placed in a ceramic crucible, and the precursor is surrounded by a protective atmosphere, such as nitrogen or an inert gas, and then the precursor is heated to a first temperature, for example 800 degrees Celsius, under a protective atmosphere. And continuing to calcine for a second time, such as but not limited to at least 7 hours, to effect heat treatment of the precursor.
  • a finished powder of the battery composite material to be prepared by the present invention that is, lithium iron manganese phosphate, having a chemical formula of LiFe x M ni - 0 4 is formed .
  • the manganese source contained in the precursor diffuses into the iron source, and the manganese source surrounds and coats the iron source in a partial substitution manner, thereby avoiding the agglomeration effect of the finished powder during the heat treatment process and improving the battery. Electrical performance. Further, the particle size of the finished powder obtained by the production method of the present invention is similar to the particle size of the iron compound as a raw material, and therefore, the stability of the product can be improved while improving the electrical properties of the battery.
  • the ratio of iron to manganese in the battery composite material synthesized in step S400 is determined, and therefore, the battery having ideal electrical properties can be prepared according to actual needs.
  • Composite material
  • fructose can be substituted with 12% by weight of lactose and 88% by weight of fructose.
  • the second product solution was ground in a ball mill and continuously milled at 450 to 650 rpm for one hour to form a precursor solution of lithium iron phosphate (LiFe x M ni — x P04).
  • the precursor solution is dried to obtain a preliminary dried precursor.
  • the dried precursor is placed in a ceramic crucible, and the precursor is subjected to at least 7 hours and above 800 degrees Celsius under a protective atmosphere. The calcination process produces a finished powder.
  • Fe 7 (P0 4 ) 6 of Example 1 was substituted with LiFePO 4 and the arrangement of other reactants was adjusted accordingly.
  • First take 118.32 grams of LiFeP0 4 and 2 liters of deionized water to mix and stir well, then add 85% by weight of phosphoric acid (H 3 P0 4 ) 264. 4 grams, the phosphoric acid can also be selected At a concentration of 85% by weight or more, after stirring uniformly, manganese carbonate (MnCO 3 ) is further added to carry out a reaction to form a first product solution.
  • MnCO 3 manganese carbonate
  • the first product solution was continuously stirred for 24 hours to fully react, and then, 13.1 g of lithium hydroxide (LiOH), 54 g of fructose, and 0.06 g of Triton X-100 were added to the first product.
  • a second product solution is formed.
  • fructose can be substituted with 12% by weight of lactose and 88% by weight of fructose.
  • the second product solution is a ball mill Grinding was carried out and grinding was continued for one hour at a speed of 450 to 650 rpm to form a precursor solution of lithium iron phosphate (LiFe x M ni -J04).
  • the precursor solution is dried to obtain a preliminary dried precursor.
  • the dried precursor is placed in a ceramic crucible, and the precursor is subjected to at least 7 hours and above 800 degrees Celsius under a protective atmosphere.
  • the calcination process produces a finished powder.
  • Example 1 and Example 2 were analyzed by X-ray diffraction (XRD) and compared with the data of International Center for Diffraction Data (ICDD). 3 and FIG. 4, the surface topography exhibited by a scanning electron microscope (SEM) is shown in FIG. 5 and FIG. 6, respectively. As shown in FIG. 3 and FIG. 4, the data measured by X-ray diffraction of the finished powders of Examples 1 and 2 were compared with the data of LiFeo.3Mno. 7PO4 provided by the International Diffraction Center, and Raman was calculated. The displacement (Raman shift) confirmed that the chemical formula is LiFeo 0 .73P0 4 .
  • the particle size of the finished powder prepared in Example 1 was less than 100 nm on average, and the particle size of the reactant Fe 7 (P0 4 ) 6 was also less than 100 nm on average.
  • the particle size of the finished powder prepared in Example 2 is between 100 nm and 300 nm, and the particle size of the reactant LiFeP0 4 is also between 100 nm and 300 nm.
  • the particle size of the iron source is similar to the particle size of the prepared finished powder, and the particle size of the finished powder is not affected by the agglomeration phenomenon, so that it has better battery electrical performance.
  • the finished powder obtained in the first embodiment and the second embodiment was coated on an aluminum substrate, and assembled into a coin-type battery (coin cel l), and charged and discharged by a charging and discharging machine for 2 cycles and 2 Coulomb charge and discharge two cycles of electrical test, the test results are shown in Figure 7 and Figure 8, respectively, therefore, the finished powder prepared in Example 1 and Example 2 has a relatively stable charge as the positive electrode material of the battery.
  • the discharge platform has a high battery capacity, and therefore, the electrical performance of the battery can be improved by the method for preparing the battery composite of the present invention.
  • the method for preparing the battery composite material of the present invention has the advantages of diffusing into the iron source by the manganese source, avoiding the agglomeration effect between the finished powders during the heat treatment, and improving the electrical performance and stability of the battery.
  • the iron source particle size and the arrangement of the manganese source ratio are selected according to actual needs.

Abstract

L'invention porte sur un procédé de fabrication d'un matériau de composite de batterie, qui comprend au moins les étapes suivantes: la fourniture d'un composé de fer, d'un acide phosphorique, d'un composé de manganèse, d'un composé de lithium et d'une source de carbone; le mélange et le brassage du composé de fer avec de l'eau désionisée, puis l'ajout de l'acide phosphorique au mélange et le brassage pour former une première solution d'acide phosphorique, et l'ajout à la première solution d'acide phosphorique d'une première quantité fixée du composé de manganèse pour amener le composé de manganèse à réagir de manière continue avec la première solution d'acide phosphorique pendant une première période de temps, formant finalement une première solution de produit; la génération d'un précurseur à travers la réaction d'au moins la première solution de produit, la source de carbone et le composé de lithium; et le traitement thermique du précurseur pour générer le matériau composite de batterie ayant une formule chimique de LiFexMn1-xPO4, x étant supérieur à 0; le matériau composite de batterie étant apte à empêcher l'effet d'agrégation de poudres finies dans le processus de traitement thermique, améliorant ainsi les performances électriques de la batterie.
PCT/CN2014/077080 2013-05-08 2014-05-08 Matériau composite de batterie et procédé de fabrication de précurseur de celui-ci WO2014180333A1 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
CN201480022089.XA CN105409033B (zh) 2013-05-08 2014-05-08 电池复合材料及其前驱物的制备方法
CA2911458A CA2911458C (fr) 2013-05-08 2014-05-08 Procede de preparation de materiau composite de batterie et son precurseur
EP14794480.5A EP2996179A4 (fr) 2013-05-08 2014-05-08 Matériau composite de batterie et procédé de fabrication de précurseur de celui-ci
KR1020157034869A KR101787229B1 (ko) 2013-05-08 2014-05-08 배터리 복합 재료 및 이의 전구물질 제조 방법
JP2016512215A JP6239095B2 (ja) 2013-05-08 2014-05-08 電池複合材料及びその前駆体の製造方法
US14/889,418 US10236512B2 (en) 2013-05-08 2014-05-08 Preparation method of battery composite material and precursor thereof

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201361820939P 2013-05-08 2013-05-08
US61/820,939 2013-05-08

Publications (1)

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WO2014180333A1 true WO2014180333A1 (fr) 2014-11-13

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US (1) US10236512B2 (fr)
EP (1) EP2996179A4 (fr)
JP (1) JP6239095B2 (fr)
KR (1) KR101787229B1 (fr)
CN (1) CN105409033B (fr)
CA (1) CA2911458C (fr)
TW (1) TWI617074B (fr)
WO (1) WO2014180333A1 (fr)

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JP6239095B2 (ja) 2017-11-29
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CA2911458A1 (fr) 2014-11-13
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US10236512B2 (en) 2019-03-19
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